Dimethyl Sulfate → 9-Chloro-1-methyl-1,10-phenanthrolinium hydrogen sulfate

HRID 241394

反応式

HRID 241394 の反応式
[Cl:1][C:2]1[CH:15]=[CH:14][C:13]2[C:4](=[C:5]3[C:10](=[CH:11][CH:12]=2)[CH:9]=[CH:8][CH:7]=[N:6]3)[N:3]=1.[S:16]([O:21]C)([O:19][CH3:20])(=[O:18])=[O:17]>C(OCC)C>[S:16]([O-:21])([OH:19])(=[O:18])=[O:17].[Cl:1][C:2]1[CH:15]=[CH:14][C:13]2[C:4]([N:3]=1)=[C:5]1[C:10]([CH:9]=[CH:8][CH:7]=[N+:6]1[CH3:20])=[CH:11][CH:12]=2

参加物

4

反応物 2

HCID 6497Dimethyl SulfateHCID 3551932-Chloro-1,10-phenanthroline

生成物 1

HCID 866711149-Chloro-1-methyl-1,10-phenanthrolinium hydrogen sulfate収率 78%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
120 °C

実験手順

Under a stream of argon, to compound (3) (5.2 g; 24.2 mmol), dimethyl sulfate (22.1 g; 175 mmol) was added at room temperature over 10 minutes. The reaction temperature was raised to 120° C. and the resulting reaction mixture was stirred for 1 hour and then cooled to room temperature. Diethyl ether was added thereto and light brown crude crystals which precipitated out were separated by filtration. The obtained crude crystals were washed with a solution of diethyl ether/ethanol=1/1 to 1/2 and dried under reduced pressure to give 6.17 g of the title compound (4).

後処理

  1. customthe resulting reaction mixture
  2. temperaturecooled to room temperature
  3. customlight brown crude crystals which precipitated out
  4. customwere separated by filtration
  5. customThe obtained crude crystals
  6. washwere washed with a solution of diethyl ether/ethanol=1/1 to 1/2
  7. customdried under reduced pressure

出典と根拠

ORDレコード
ord-2773828520054e6eba5b514301b77560
出典データセット
uspto-grants-2014_02
特許番号
US08648194B2

関連ノート

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